Micellar Electrokinetic Chromatography of Cephalosporin Antibiotics

A simple micellar electrokinetic chromatographic (MEKC) method is described for the simultaneous separation of twelve cephalosporin antibiotics. The separation was performed in a phosphate buffer (0.1 M, pH 6.6) with sodium dodecyl sulfate (SDS) (0.1 M) as an anionic surfactant. The complete separation of twelve cephalosporins was attained in 36 min. Application of the method to the quantitative analysis of cefuroxime, cephalexin, cephapirin and cephradine in pharmaceutical preparations was demonstrated.     

毛细管胶束电动色谱法分析PTH氨基酸

建立了用毛细管胶束电动色谱法（MEKC）分离19种PTH氨基酸的方法,并探讨了电压、pH值、温度、胶束浓度对氨基酸迁移时间的影响。方法具有速度快、灵敏度高、样品用量少的优点。     

毛细管胶束电动色谱法分离测定胆红素亚组分

用毛细管胶束电动色谱法成功地分离和定量测定了血清及胆汁中α，β，γ及δ等４种胆红素亚组分。二牛磺酸胆红素浓度在５１０μｍｏｌ／Ｌ以下时，峰面积与浓度呈良好的线性关系，二牛磺酸胆红素浓度即使为１．５μｍｏｌ／Ｌ时仍可检测出明显的定量峰。用一份２５５μｍｏｌ／Ｌ的二牛磺酸胆红素标准液进行重复性检测，第１次定量结果为２６０μｍｏｌ／Ｌ，出峰时间１６ｍｉｎ；第５０次电泳结果为２３８μｍｏｌ／Ｌ，出峰时间１６．７ｍｉｎ。     

胶束电动毛细管色谱分离氨基酸和磷酸化氨基酸

本文报道了胶束电动毛细管色谱分离、汞灯诱导荧光电荷耦合器件检测分析氨基酸和磷酸化氨基酸的 4-氟 - 7-硝基苯 - 2 - 口恶 - 1 ,3-丫唑衍生物。研究表明 ,在 p H9.35的 1 0 mmol/L硼砂和 1 0 mmol/L十二烷基硫酸钠的电泳缓冲介质中 ,5种氨基酸和 3种磷酸化氨基酸在 1 0 min内完全分离 ,检测灵敏度为 1 .2 1× 1 0 - 8～ 5 .2 1×1 0 - 8mol/L ,分离效率达 7.3× 1 0 5～ 3.0× 1 0 5/m理论塔板数 ,结果令人满意     

咖啡因及其9种类似物的胶束电动毛细管分析研究

 以十二烷基硫酸钠 (SDS)胶束为准固定相 ,考察了咖啡因及其 9种类似物在胶束电动毛细管 (MECC)分离模式下的分离行为。研究了运行缓冲液的 pH值、磷酸盐浓度、SDS浓度、甲醇体积分数、分离电压、分离温度等因素对这 10种化合物的迁移时间和分离效果的影响。结果发现 ,这些因素对上述 10种化合物的分离有显著的影响 ,尤以pH值为最。它不仅影响化合物的迁移时间和分离效率 ,还改变其出峰顺序 ,这与碱性条件下化合物仲胺基上氢的电离有关。优化后的分离条件 :运行缓冲液为 2 0mmol/L磷酸盐 2 0mmol/LSDS(pH 11 0 ) ,分离电压为2 5kV。     

Separation of Aniline Derivatives by Micellar Electrokinetic Capillary Chromatography

A micellar electrokinetic capillary chromatography (MECC) was developed for the determination of aniline and 6 substituted anilines. The seven components were separated within 25min in the buffer solution of 40mmol/L sodium borate and 100mmol/L SDS. It was found that the separation was dependent on operating voltage, pH value, borate and SDS concentrations.The analytical performance was examined in terms of linear response and reproducibility.Wastewater was determined by the established method.     

电动胶束色谱中弱酸性化合物的柱上浓缩富集技术的研究

提出一种电动胶束色谱（ＭＥＫＣ）中弱酸性化合物的柱上浓缩富集技术,并得到实验证实。以七种弱酸性巴比妥类药物的ＭＥＫＣ分离为例,考察了样品溶剂中表面活性剂浓度、ｐＨ值和离子强度等对富集作用的影响。表面活性剂浓度,ｐＨ值对富集效应的影响较大。采用低浓度（略高于ＣＭＣ点）表面活性剂、低浓度缓冲液作样品溶剂,调节溶剂ｐＨ值小于待测化合物的ｐＫａ－１,就可以对弱酸性化合物进行柱上富集。采用这种富集技术,可以压缩样品带的宽度从而提高柱效,在此基础上可通过加大进样量提高化合物的检测灵敏度。     

单纯形算法动态优化毛细管胶束电动色谱分离体系

采用控制加权可变步长单纯形算法对ＰＴＣ氨基酸的毛细管胶束电动色谱分离体系进行动态优化。寻优过程中同时考虑背景电解质的ｐＨ值、十二烷基硫酸钠浓度和有机添加剂浓度对体系分离效果的影响。分别使用Ｌｏｎｇ系数法和均匀设计表法确定初始单纯形顶点对分离体系进行动态优化。优化结果使１７种ＰＴＣ氨基酸获得了比较满意的分离。     

月桂酸胶束电动毛细管色谱快速分离三嗪类农药的研究

以月桂酸为表面活性剂和三羟甲基氨基甲烷(Tris)组成缓冲溶液,建立了毛细管胶束电动色谱快速测定8种三嗪类农药的方法.对电泳介质的种类及浓度、pH值、操作电压和进样时间等影响因素进行了优化,在以50 mmol/L月桂酸和100 mmol/L Tris作为缓冲溶液(pH 10.0)、体积分数为20%的丙酮作有机改性剂的条件下,可以在2.2 min内实现对嗪草酮、氰草津、西草津、莠去津、扑灭通、莠灭净、扑灭津、特丁净的分离检测.结合固相萃取(SPE)对农田水样进行测定,各农药检出限为0.5～2.5μg/L,回收率为88%～106%,相对标准偏差为3.3%～5.0%.     

Micellar Electrokinetic Chromatography of X-Ray Film Developing Baths

A simple and fast micellar electrokinetic chromatographic (MEKC) method for the determination of five main compounds (hydroquinone, metol, phenidone, 2-hydroxy-5-methylaminobenzenesulphonate and 2,5-dihydroxybenzenesulphonate) in X-ray film developing solutions was developed. The optimal conditions for the separation were established by varying the concentration of sodium dodecyl sulfate (SDS), the electrolyte pH and the temperature. Successful results were obtained with a 25mmolL^–1 Tris-phosphate buffer at pH 9.0 in the presence of 50mmolL^–1 SDS using direct UV detection at 214nm. Under these conditions, baseline separation of the five compounds was achieved in less than 8min. The method was validated in terms of precision, linearity, accuracy, and successfully applied to the analysis of X-ray film developing baths.     

咔唑-9-乙基氯甲酸酯柱前衍生氨基酸胶束电动色谱分离

采用一种新型紫外、荧光衍生试剂咔唑-9-乙基氯甲酸酯对9种氨基酸(丝氨酸、苏氨酸、甘氨酸、谷氨酸、天冬氨酸、缬氨酸、异亮氨酸、亮氨酸、苯丙氨酸)进行柱前衍生,采用胶束电动色谱模式在14 min内完成分离。分离条件：以pH 9.0的 20 mmol/L硼酸盐-30 mmol/L十二烷基硫酸钠(SDS)溶液（含3%(体积分数)乙腈)为缓冲溶液,柱温25 ℃,分离电压18 kV,紫外检测波长214 nm。该方法的线性范围为0.025~0.25 mmol/L,检出限为2.15~2.46 μmol/L。     

胶束毛细管电动色谱法用于祖师麻中5种主要成分的测定

采用胶束毛细管电动色谱法分离和测定祖师麻中紫丁香苷(SR)、7-甲氧基香豆素(7-MC)、瑞香苷(DN)、瑞香素(DP)和7-羟基香豆素(7-HC)等5种组分,通过研究影响分离和测定的主要因素,建立一种快捷、简便的方法用于5种组分的分离测定.在最佳电泳介质(10 mmol/L SDS pH=9.0,20 mmol/L硼酸盐缓冲溶液)中,5种待测组分在8 min内实现基线分离.SR、7-MC、DN、DP和7-HC的线性响应范围分别为1.0~100、1.5~100、5.0~75、5.0~75和1.0~75!g/mL;检测限分别为0.3、0.5、1.7、1.7和0.3!g/mL.方法成功应用于实际样品祖师麻注射液及祖师麻片中SR、7-MC、DN、DP和7-HC的含量测定.     

胶束电动力学毛细管色谱中峰的定性方法

从理论上探讨了在胶束电动力学毛细管色谱中采用迁移时间来定性的不足，提出将相对有效淌度用于该体系下尿中核苷组分的定性。结果表明：使用相对有效淌度作定性指标，其平均相对标准偏差为1．54％，明显优于同迁移时间进行定性所得的平均相对标准偏差7．9％。提出用识别系数评价定性的可靠性。当使用相对有效淌度作定性指标时，75％以上的分析物都达到了可靠识别。识别可靠性与采用迁移时间相比最高可提高16倍。     

Fast and High-Performance Screening of Narcotic Drugs on a Microfluidic Device by Micellar Electrokinetic Capillary Chromatography

This work presents a new approach for fast and sensitive ultraviolet detection of 12 kinds of narcotic drugs on a microfluidic device by micellar electrokinetic capillary chromatography. Under optimal sampling and separation conditions the baseline separation of 12 drugs with resolution values ranging from 1.06 to 4.04 and separation efficiency up to 5.14 × 10⁵ plates m^?1 was achieved within 200 s. The widest linear range for detection of these analytes was 1.0 to 1500.0 µg mL^?1. The correlation coefficients are higher than 0.9994. This system can successfully be applied to analyze narcotic drugs in human urine with the aid of liquid-liquid extraction of the samples. This method allows minimum detectable concentrations of these drugs down to 33 ng mL^?1 at a signal-to-noise ratio of 3. This rapid method with high resolution and sensitivity, and little solvent consumption possessed potential application in screening of narcotic drugs in forensic analysis.     

Bile Salts in Chiral Micellar Electrokinetic Chromatography: 2000–2020

Bile salts are naturally occurring chiral surfactants that are able to solubilize hydrophobic compounds. Because of this ability, bile salts were exploited as chiral selectors added to the background solution (BGS) in the chiral micellar electrokinetic chromatography (MEKC) of various small molecules. In this review, we aimed to examine the developments in research on chiral MEKC using bile salts as chiral selectors over the past 20 years. The review begins with a discussion of the aggregation of bile salts in chiral recognition and separation, followed by the use of single bile salts and bile salts with other chiral selectors (i.e., cyclodextrins, proteins and single-stranded DNA aptamers). Advanced techniques such as partial-filling MEKC, stacking and single-drop microextraction were considered. Potential applications to real samples, including enantiomeric impurity analysis, were also discussed.     

表面活性剂作为电解液添加剂在毛细管电泳中的应用

本综述归纳了近年来毛细管电动色谱的理论研究，以及阴离子、阳离子和非离子表面活性剂的应用研究工作，并介绍了毛细管电动色谱的改良新技术，如环糊精、胆汁盐，其它旋光异构体选择及有机溶剂等作为添加剂的应用，引用文献１７４篇。     

毛细管胶束电动色谱测定解热镇痛药成份

用毛细管胶束电动色谱对解热镇痛药的有效成份进行了分离和定量研究,实验在自装的毛细管电泳装置上进行。考察了电压及胶束溶液浓度对分离的影响,峰面积定量的重现性及线性。用二点内标法分析去痛片中的咖啡因、苯巴比妥、氨基比林、非那西汀。测定结果与HPLC结果一致。     

苯胺类化合物的胶束电动毛细管色谱优化分离

研究了用胶束电动毛细管色谱分离对-氯苯胺、对-溴苯胺、2,4-二氯苯胺、对-碘苯胺;在选定的实验条件下,各化合物迁移时间的相对偏差(RSD)＜0.5%,峰面积RSD＜3.0%,苯胺化合物的检出限为(1.2～4.2)×10-6mol/L;方法用于实验室废水分析,结果令人满意.     

Roles of Organic Modifiers in Micellar Electrokinetic Capillary Chromatography

In the present work, four organic modifiers, viz. urea, dioxane, methanol, and tetrahydrofuran, were comparatively and systematically studied in terms of their effects on electrokinetic migration behavior and the retention mechanism of homologous solutes in MECC. The results showed that the electroosmotic mobility, μ_eo, and the electrophoretic mobility of a micelle, μ_ep,mc, decrease linearly with increasing organic modifier concentration. The ability of organic modifiers to lower μ_eo is greater than their ability to lower μ_ep,mc. The negative values of the slopes of these linear relationships, D_eo and D_ep,mc, increase along the series the order urea < methanol < dioxane < tetrahydrofuran. The logarithm of the capacity factor (ln k′) of uncharged homologous solute, which is mainly determined by the hydrophobic interaction, decreases linearly with increasing organic modifier concentration, due not only to the decrease in the partition coefficient but also to the decrease in the phase ratio. A linear relationship was observed between the slope of the plot of ln k′ vs. organic modifier concentration and the carbon number of homologous compound. The slope of such a relationship can characterize the hydrophobicity of the organic modifier. The hydrophobicity of such organic modifiers is also found to increase along the series urea < methanol < dioxane < tetrahydrofuran.